Process of manufacturing nitrogen compounds.



H. PETTIBONE & VB. VON SHOLLY. PROCESS OF MANUFACTURING NITROGEN COMPOUNDS. APPLICATION FILED AUG. 19, 1908.

1,042, 141 Patented Oct. 22, 1912.

witnesses the'heat units have been utilized for prodown-draft gas'generator A, having a top.

' chamber B, grate b andthe usual ash pit.

unrrln STATES PATENT new mom, or new nocnE Ln, AND BEHJAMIN Von SHOLLY, or rnn'smne,

- new YORK.

inociiss or manunecrunme-nrrnoenncomrounns.

Specification of Letters Patent.

Patented 0ct. 22,"191 2.

Application filed August 19, 1968. Serial Il'o. 449,310.

residing at New Rochelle, in the county of Westchester, State of New York, and

BENJAMIN VON SHoLLY, residing at Flush ing, in-the county of Queens and State of New York-citizens of the United States, have invented certain new and useful Im-" provementsz in-Processes of Manufacturing Niimpgen Compounds, of which the, follow ingls a specification.

The object of our invention is to provide an economical and effective method of manufacturing cyanamid andother nitrogen compounds, and at the same time utilize a lay-product in. the nature of spent gas, after duction of heat or power.

A special object of our invention is to provide for the production and utilizationof cheap nitrogen in the manufacture of cy-v anamid, whereby great economy isefi'ected in obtaining the product.

The matter constituting our invention will be defined in the claims.

We will now describe our process and one form of apparatus for carrying-it out, by

referenceto the accompanying drawings, 1n Y whichp I Figures 1 and 1? represent diagrammatically, partly in elevation and partly in section, our apparatus. i I We preferably use a Loomis Pettibone fuel opening and tight fitting lid 01, a'fuel A hot air supply pipe C connects the hot air rhamber of a tubular air-heater or economizer E with the top of the generator, and a gasoutlett pipe D connects the ash-pit with the lower gas chamber (1 of the heater; A gas scrubber Fis connected by a pipe and valve .9 with the upper gas chamber d and at its lower end is connected by pipe f with a combined exhaust fan and centrifugal extractor G. A pipe F having a valve, may lead from gaschamber d'directly to the fan and extractor in case the scrubber is not required.

The exhaust fan and extractor deliver the gas by pipe g into a small holder H, or by a bypass pipe g, having a valve, directly to the inlet pipe of a" burner in the retort furnace. An outlet pipe it, hav ng a valve 5 2;, connects theholder with a T coupling Z which connects pipe n with a burner a holder V for nitrogen gas.

ing the gas through the heating coil.

' in t'he ruinac''o. air-blower L connects by its discharge pipe and valve m with the good gas and air mixing burner, producing perfect combustion, can be used.

In thefurnace O'are placed the combining retorts P, preferably through retorts, having mouth-pieces at each end, of'which four may be conveniently" used. A take-off pipe R for products of'combustion connects with T coupler Z leading .tothe burner N. Any

the top of the furnace and with a jet .ex-' hauster 'S (see Fig. 1*), having .a fluid 'sup--.

or other material for removing carbonic ac1d and sulfur compounds from the gaseous products. -Any purifying material .best

adapted for the purpose-will be'used','also any desired kindof purifying apparatus.

An outlet pipe 21. connects the purifier with.

leads from the holder and connects with the retorts by branch pipes and valves y 'connecting with the mouth-pieces. e preferably connect a branch pipe lV fwithpipe W and pass it into furnace'O- and thereconnect it with a recuperative device, suc'lf as heat ng e011 V located 1n the top above the retorts' as shown, or other convenient part A pipe of the furnace This coil connects with the,

delivery end of pipe WV. and the latter is provided with a shut-0E valve 00 for direct- Theoutlet pipes :27 connecting withthe mouthpieces at the other ends of the retorts may. also be connected with the coil as indicated by dotted lines, or with a separate heater,

so that nitrogen gas may be heated and cir-. T

'culated through the-retorts and heater for maintaining the desired temperature of the material undergoing. treatment;

The jet-exhauster S will, in practice, he an automatic regulating jet exhauster, which will tend to maintain a slightly di min'ished pressure in the fire chamber and force the gaseous products through the scrubber and purifier into the second gas holder V.

The operation of making cyanamid is very simple and may be conducted-asfollows: Fire is kindled in the generator and a gcodproducer gas generated fromllquid O .2 CO 26. 0 CHy 1.3 H 9.0 2 60. O

. 100.0 (H S traces, $0,. trades, water vapor.)

A store of gas having been accumulated, it is admitted to the burner Y, together with a regulated air supply, and ignited, the proportions of gas and air being regulated to produce perfect combustion without material excess of either gas or air in the chamber around the retorts P. The resulting products of combustion are substantially free of both air and unburnt gas,- containing approximately the following constituents C0 16.3 O er. 0. 2 CO 5 N 83. 0 H O trace SO traces.

absorbed by the purifying material The purified gas, consisting of nitrogiii, 9t .3 per cent. and other gases, seven tenths of one per cent, is stored in the holder V, from which it is supplied to the retorts as re quired.

The retorts being heated a red heat, approximately 800 (3., arecharged with carbids and halogen salts, mixed in suitable proportions, introduced at the rear ends, and the lids tightly closed. The carbids and halogen salts being heated to the proper temperature the valves 3 are opened, admitting nitrogen which has been preheated in the coil and which passing in contact with the red hot charge causes a chemical reaction to take place between it and the carbidmixture wh ch is expressed by the following equatiom using calcium carbid as an example: CaC +N CaNCN+G of our cool nitrogen gas, and a fresh charge an atmosphere I of carbid mixture introduced and the proc-.

ess repeated.

Operating in the described manner, the

source of heat for the retorts also furnishes thenitrogen which is necessary and furnishes it so cheaply that a continuous stream of the substantially purenitrdgen gas can be run through the retort,- malntaining amaximum richness in nitrogen of the atmosphere therein. Both-the nitrogen of the producer gas and the heat ofcombustion. In the walled space around the retort" ercise of some care the produ be burned with the exact qua, needed for combustion, furnishing an efiluent which is, as shown by the cited analysis, substantially entirely composed of carbon dioxid and nitrogen. Upon removal of the former, substantially pure nitrogen is left. In the cyanamid reaction this pure gas is very desirable since it either carbon dioxid or'carbon'monoxid be present in substantial amount wasteful side-reactions occur. In

other words, in operating in the described manner both the necessary heat and the necessary nitrogen are attained together.

Among the advantages of'our process of producing cyana'mids are the following A cheap and rapid method of producing substantially pure nitrogen and utilizing, for its production, the waste products of a previous operation used in the process.

By using gas for heating the retorts, we are enabled to maintain any required te1nperature, and" uniformly heat the retorts throughout their entire lengths, It also permits of an intimateadmixture of a suitable proportion of air with the gas to effect complete combustion without using any excess of oxygen, so that the products of C0111- bustion will contain the maximum percentage of nitrogen. This result cannot be at tained with other forms of fuel.

Ve alsohave the advantage of quickness, convenience and cleanliness of operation.

Our process may be modified by consuming the gas from the generator in, an internal combustion engine, which is used foroperating a dynamo to generating electric current, this current being used to produce an are for the manufacture of carbid. Theexhaust gaseous products from theengine will be cleaned, and purified and the resultnitrogen of the air used to burn ltare utilized, as well zas the I.

-' ing nitrogen stored in aholder, and passed,

1 pound which as required through the carbid during its Patent, is=

' 1. The process of making nitrogen com pounds which comprises heating a substance 'able to take up nitrogen in a retort, by burning producer gas with substantially the theoretical' amount of air aroundsaid retort to furnish the heat, removing carbon dioxid 25 from the product of combustion to furnish nitrogen and transmitting said freed nitrogen to the interior of the retort to combine.

with said substance.

2. The process of making a nitrogen comcomprises heating calcium carbid in a retort, by burning producer gas with substantially the theoretical amount of air around said retort to furnish the heat, removing carbon dioxid from the product cf'combustion to furnish nitrogen and transmitting said freed nitrogen to the interior of the retortin contact with said carbid.

3. The process of making a nitrogen compound which comprises heating a substance able to take up nitrogen in a retort, by burnping producer gas with substantially the theoretical amount of air around the'retort to furnish the heat, removing carbon dioxid hori zontal retorts are shown we v our invention, what we claim as new. and desire to secure by Letters such carbid,

from the product of combustion to furnish nitrogen, reheating thefreed nitrogen and transmitting it to the interior. of the retort in contact with said substance.

. 4. The process of making a nitrogen compound which comprises heating calcium car- 'bidin a'retort, by burning producer 'gas with substantially the theoretical amount of air around the'retort to furnish the heat, re-. moving carbon dioxid from the product'of' combustion to furnish freed nitrogen, reheating the nitrogen and transmitting it to the interior of theretort in contact with said carbid.

5. The-process of making cyanamid which comprises heating calcium carbid in a retort with the aid of producer gas burning there-- around with substantially the theoretical amount of air, passing the products of combustion in contact with lime to remove carbon dioxid and furnish substantially pure nitrogen and returning such freed nitrogen to the interior of the retort to react with 6, The process; of producing nitrogen compounds,- which consists in simultaneously utilizing the heat and nitrogen resulting from the combustio'n of a gaseous fuel in connection with a reacting substance, such as calcium c'arbid, by first burning the fuel gas for highly heatingthereacting sub;

stance, then separating the nitrogen from the resulting product and passing such free nitrogen incontact with the heated reacting substance.

In testimony whereof we afiix our signatures in presence oftwo witnesses.

HAVVLEY PETTIBONE. BENJAMIN VON SHOLLY. Witnesses:

W. R. FULLER, H. A. KIMBER. 1 

